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目的建立蜂蜜中掺假的快速鉴定方法。方法将蜂蜜样品溶解后进行真空干燥,然后对样品中的低聚糖进行荧光标记,以氨基柱为分析柱,采用乙腈和甲酸铵为流动相,对标记低聚糖进行高效液相色谱分离,采用ESI-MS的SIR模式对标记低聚糖进行定性测定。结果基于荧光标记试剂2-氨基苯甲酰胺(2-AB)和毒性较低的还原剂2-甲基吡啶-N-甲硼烷(2-PB)的还原氨化反应能有效地对蜂蜜中的带还原端的低聚糖进行荧光标记。天然蜂蜜含有单糖(DP1)、双糖(DP2)和少量三糖(DP3),掺假蜂蜜除此以外还含有少量四糖(DP4)、五糖(DP5)和六糖(DP6)。结论采用此法对蜂蜜样品进行蜂蜜掺假判定与国标方法测试结果基本吻合,而且不需对样品进行净化处理即可上机分析,为建立蜂蜜掺假的快速筛查方法提供参考。
Objective To establish a rapid identification method of adulteration in honey. Methods The sample of honey was dissolved and dried under vacuum. Then, the oligosaccharides in the sample were labeled by fluorescence. Amino columns were used as the analytical column. Acetonitrile and ammonium formate were used as the mobile phase. The labeled oligosaccharides were separated by high performance liquid chromatography (HPLC) Qualitative determination of labeled oligosaccharides was performed using the SIR mode of ESI-MS. Results The reductive amination reaction based on 2-aminobenzamide (2-AB), a fluorescent labeling reagent, and 2-picoline-2-borane (2-PB), a less toxic reducing agent, Of the oligosaccharides with the reducing end were fluorescently labeled. Natural honey contains monosaccharide (DP1), disaccharide (DP2) and a small amount of trisaccharide (DP3). Adulterated honey also contains small amounts of DP4, DP5 and DP6. Conclusions The method of adulteration of honey adulterated with this method is in good agreement with that of the national standard method, and it can be analyzed on the machine without the need of purification treatment, which can provide a reference for the establishment of rapid screening method of honey adulteration.